Separations最新文献

{"title":"Determination of Topiramate and Carbamazepine in Plasma by Combined Dispersive Liquid–Liquid Microextraction and Gas Chromatography–Mass Spectrometry","authors":"P. Cabarcos-Fernández, M. Tabernero-Duque, I. Álvarez-Freire, A. Bermejo-Barrera","doi":"10.3390/separations11020051","DOIUrl":"https://doi.org/10.3390/separations11020051","url":null,"abstract":"Dispersive liquid–liquid microextraction, an environmentally friendly extraction technique, followed by gas chromatography–mass spectrometry operating in selected ion monitoring (SIM) mode, is here presented for the simultaneous determination of two anticonvulsant drugs in plasma, Topiramate and Carbamazepine. Experimental parameters affecting the recovery of the proposed extraction method, such as the extraction and dispersion solvent, the extraction and dispersion volume, the sample amount, the pH of the aqueous phase, the ultrasound time, the centrifugation time and ionic strength, were investigated. The limits of detection for Topiramate and Carbamazepine were 0.01 and 0.025 µg mL−1, and the limits of quantification were 0.025 µg mL−1 and 0.05 µg mL−1, respectively. The method is shown to be selective, accurate, precise and linear over the concentration ranges of 0.025–8 µg mL−1 for Topiramate and 0.05–3 µg mL−1 for Carbamazepine. The extraction recovery of the analytes ranged from 91.5% to 113.9%. The analytical method was successfully applied to real plasma samples received by the Forensic Toxicology Service of the Forensic Science Institute of Santiago de Compostela.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"60 1-2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139855970","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of Topiramate and Carbamazepine in Plasma by Combined Dispersive Liquid–Liquid Microextraction and Gas Chromatography–Mass Spectrometry","authors":"P. Cabarcos-Fernández, M. Tabernero-Duque, I. Álvarez-Freire, A. Bermejo-Barrera","doi":"10.3390/separations11020051","DOIUrl":"https://doi.org/10.3390/separations11020051","url":null,"abstract":"Dispersive liquid–liquid microextraction, an environmentally friendly extraction technique, followed by gas chromatography–mass spectrometry operating in selected ion monitoring (SIM) mode, is here presented for the simultaneous determination of two anticonvulsant drugs in plasma, Topiramate and Carbamazepine. Experimental parameters affecting the recovery of the proposed extraction method, such as the extraction and dispersion solvent, the extraction and dispersion volume, the sample amount, the pH of the aqueous phase, the ultrasound time, the centrifugation time and ionic strength, were investigated. The limits of detection for Topiramate and Carbamazepine were 0.01 and 0.025 µg mL−1, and the limits of quantification were 0.025 µg mL−1 and 0.05 µg mL−1, respectively. The method is shown to be selective, accurate, precise and linear over the concentration ranges of 0.025–8 µg mL−1 for Topiramate and 0.05–3 µg mL−1 for Carbamazepine. The extraction recovery of the analytes ranged from 91.5% to 113.9%. The analytical method was successfully applied to real plasma samples received by the Forensic Toxicology Service of the Forensic Science Institute of Santiago de Compostela.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"9 11","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139795999","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A New Ultra High-Performance Liquid Chromatography-Tandem Mass Spectrometry Method to Monitor 1-Amino-4-Methyl-Piperazine and 1-Methyl-4-Nitroso-Piperazine in Rifampicin Hydrolysis: A Standard Addition Approach to Quantify Nitrosamine in Rifampicin","authors":"Alessia Panusa, Paola Rotundo, Daniele Sadutto, Andrea Rodomonte, R. Cirilli","doi":"10.3390/separations11020054","DOIUrl":"https://doi.org/10.3390/separations11020054","url":null,"abstract":"1-amino-4-methyl-piperazine (AMP) is both a starting material for the synthesis of rifampicin (RIF) and a degradation product of RIF hydrolysis. 1-methyl-4-nitroso-piperazine (MNP) is an oxidation product of AMP as well as a potentially genotoxic N-nitrosamine. The EMA and FDA have approved an ad interim limit of 5 ppm for MNP in RIF drug products. As in-house methods for the analysis of MNP in RIF use a wide range of conditions for mobile phases and sample diluents, we decided to investigate whether these conditions affect the formation of MNP and AMP. A UHPLC-MS/MS method was developed to simultaneously quantify AMP and MNP during RIF hydrolysis in buffered aqueous solutions at different pH levels. Analyses were performed in MRM mode; separations were carried out on an InfinityLab Poroshell HPH-C18 (100 mm, 2.1 mm i.d., particle size 1.9 μm). In aqueous RIF solutions, the content of AMP and MNP increases with time; at different pHs, the concentration of AMP increases much faster in acidic than in basic solutions; and the increase in MNP can be reduced by the addition of ascorbic acid. To avoid an overestimation of MNP, water should not be used as a diluent in RIF sample preparations. Methanol is a more suitable diluent than water. A standard addition method has been validated for the quantification of MNP in RIF drug substances.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"37 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139854893","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Analysis of the Lipid Component and the Sterol Ester Fraction for the Detection of Soft Wheat in Durum Wheat Flour and Pasta","authors":"D. Naviglio, Angela Perrone, Francesca Varchetta, P. Trucillo, D. Montesano, M. Gallo","doi":"10.3390/separations11020053","DOIUrl":"https://doi.org/10.3390/separations11020053","url":null,"abstract":"Food adulteration consists of changing the original structure of a food, and so, by its definition, it is a process not admitted by law. Adulterations can not only have commercial consequences, but also hygienic and nutritional ones, and in some cases, they can cause a serious danger to public health. Therefore, it is of great interest to understand and identify the modifications that alter the original chemical composition of a food item (nutrition label). Among the food processing sectors, the pasta food chain is a fascinating production process, which finds its roots in a mixture of a few, simple ingredients; in particular, in its basic formulation to produce pasta, exclusively durum wheat mixed with water is used, while soft wheat and therefore the flour obtained from it are destined for bakeries and the confectionery industry. In this work, a procedure was developed that allows the detection of the possible presence of soft wheat in durum wheat-based products, both in the flour and after the pasta-making process. It is to point out that this adulteration is only commercial fraud and there are no consequences for people’s health. In detail, the method was based on the isolation of the lipid fraction of flours and pastas and using the gas chromatographic analysis of the sterol ester fraction, which were not altered during the pasta-making phase, because they have very high boiling points. Based on the evaluation of some specific ratios between sterol esters, it was possible to trace the percentage of soft wheat present in a mixture with durum wheat, both in flour products and pastas.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"43 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139855077","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A New Ultra High-Performance Liquid Chromatography-Tandem Mass Spectrometry Method to Monitor 1-Amino-4-Methyl-Piperazine and 1-Methyl-4-Nitroso-Piperazine in Rifampicin Hydrolysis: A Standard Addition Approach to Quantify Nitrosamine in Rifampicin","authors":"Alessia Panusa, Paola Rotundo, Daniele Sadutto, Andrea Rodomonte, R. Cirilli","doi":"10.3390/separations11020054","DOIUrl":"https://doi.org/10.3390/separations11020054","url":null,"abstract":"1-amino-4-methyl-piperazine (AMP) is both a starting material for the synthesis of rifampicin (RIF) and a degradation product of RIF hydrolysis. 1-methyl-4-nitroso-piperazine (MNP) is an oxidation product of AMP as well as a potentially genotoxic N-nitrosamine. The EMA and FDA have approved an ad interim limit of 5 ppm for MNP in RIF drug products. As in-house methods for the analysis of MNP in RIF use a wide range of conditions for mobile phases and sample diluents, we decided to investigate whether these conditions affect the formation of MNP and AMP. A UHPLC-MS/MS method was developed to simultaneously quantify AMP and MNP during RIF hydrolysis in buffered aqueous solutions at different pH levels. Analyses were performed in MRM mode; separations were carried out on an InfinityLab Poroshell HPH-C18 (100 mm, 2.1 mm i.d., particle size 1.9 μm). In aqueous RIF solutions, the content of AMP and MNP increases with time; at different pHs, the concentration of AMP increases much faster in acidic than in basic solutions; and the increase in MNP can be reduced by the addition of ascorbic acid. To avoid an overestimation of MNP, water should not be used as a diluent in RIF sample preparations. Methanol is a more suitable diluent than water. A standard addition method has been validated for the quantification of MNP in RIF drug substances.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"96 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139794779","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Content of Acidic Compounds in the Bean of Coffea arabica L., Produced in the Department of Cesar (Colombia), and Its Relationship with the Sensorial Attribute of Acidity","authors":"Luz Fanny Echeverri-Giraldo, Valentina Osorio Pérez, Claudia Tabares Arboleda, Lady Juliet Vargas Gutiérrez, Luis Carlos Imbachi Quinchua","doi":"10.3390/separations11020052","DOIUrl":"https://doi.org/10.3390/separations11020052","url":null,"abstract":"Cesar, a coffee-growing department in Colombia, has particular characteristics that favor the production of coffees differentiated by sensory profile, for which the acidity attribute stands out. The chemical composition and sensory quality of the coffee produced by 160 coffee growers during two production harvests (2021 and 2022) and processed by the wet method were evaluated to correlate the contents of the main acidic chemical compounds present in green coffee beans with the perceived acidity of the beverage. The chemical analysis of coffee samples utilized spectrophotometric methods and HPLC-DAD techniques. Lactic, 3,5-di-CQA and phosphoric acids were good discriminators of acidity classified as excellent; that is, with a score higher than 7.75 on the Specialty Coffee Association (SCA) scale, presenting the highest contents in the green coffee bean. There was a direct linear relationship between acidity and 3,5-di-CQA and 5-CQA and an inverse relationship between acidity and 3-CQA, 4-CQA and 4,5-CQA. These findings contribute to the understanding of the quality and chemistry of Colombian coffee.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"23 31","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139796052","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Analysis of the Lipid Component and the Sterol Ester Fraction for the Detection of Soft Wheat in Durum Wheat Flour and Pasta","authors":"D. Naviglio, Angela Perrone, Francesca Varchetta, P. Trucillo, D. Montesano, M. Gallo","doi":"10.3390/separations11020053","DOIUrl":"https://doi.org/10.3390/separations11020053","url":null,"abstract":"Food adulteration consists of changing the original structure of a food, and so, by its definition, it is a process not admitted by law. Adulterations can not only have commercial consequences, but also hygienic and nutritional ones, and in some cases, they can cause a serious danger to public health. Therefore, it is of great interest to understand and identify the modifications that alter the original chemical composition of a food item (nutrition label). Among the food processing sectors, the pasta food chain is a fascinating production process, which finds its roots in a mixture of a few, simple ingredients; in particular, in its basic formulation to produce pasta, exclusively durum wheat mixed with water is used, while soft wheat and therefore the flour obtained from it are destined for bakeries and the confectionery industry. In this work, a procedure was developed that allows the detection of the possible presence of soft wheat in durum wheat-based products, both in the flour and after the pasta-making process. It is to point out that this adulteration is only commercial fraud and there are no consequences for people’s health. In detail, the method was based on the isolation of the lipid fraction of flours and pastas and using the gas chromatographic analysis of the sterol ester fraction, which were not altered during the pasta-making phase, because they have very high boiling points. Based on the evaluation of some specific ratios between sterol esters, it was possible to trace the percentage of soft wheat present in a mixture with durum wheat, both in flour products and pastas.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"10 20","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139794958","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"CO2 Adsorption by Bamboo Biochars Obtained via a Salt-Assisted Pyrolysis Route","authors":"Xing Xie, Mangmang Li, Dan Lin, Bin Li, C. Li, Dongjing Liu","doi":"10.3390/separations11020048","DOIUrl":"https://doi.org/10.3390/separations11020048","url":null,"abstract":"Recently, salt-assisted pyrolyzation has been deemed an emerging and efficient method for the preparation of biochars due to its facile operation as well as its good structural and chemical properties. In this work, biochars (MBCx) are prepared by heating bamboo powders in eutectic salts (Li2CO3 + K2CO3) at 500–600 °C in the air. Multiple technologies are employed to examine the physiochemical properties of bamboo biochars. Correlations between heating temperature and structural features and carbon dioxide uptakes of bamboo biochars have been investigated. The results show that heating temperature has a significant influence on the physicochemical properties of bamboo biochars. With the elevation of the heating temperature, the defect structures of bamboo biochars gradually ascend, especially when the heating temperature reaches 600 °C. MBCx biochars visibly exceed conventional bamboo biochar prepared via pyrolyzation in a nitrogen stream free of salt addition. Pyrolysis of bamboo in eutectic salts endows biochars with higher oxygen content and more carbon defects, which likely accounts for their better CO2 capture activities.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"37 5","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139801712","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Chemical Composition and Antistaphylococcal Activity of Essential Oil of Curcuma mangga Rhizome from Indonesia","authors":"K. Urbanova, A. Romulo, M. Houdková, P. Nový, L. Kokoska","doi":"10.3390/separations11020049","DOIUrl":"https://doi.org/10.3390/separations11020049","url":null,"abstract":"This study assessed the antistaphylococcal activity of essential oil (EO) hydrodistilled from the rhizome of Curcuma mangga grown in Indonesia using the broth microdilution volatilization method and standard broth microdilution method modified for evaluation of volatile agents, as well as described its chemical composition using gas chromatography (GC) with mass spectrometry (MS). A fused-silica HP-5MS column and a DB-17MS column were used to separate the components into two columns. The results demonstrated that the EO exhibited antistaphylococcal activity at the minimum inhibitory concentration (MIC) ranging from 128 to 1024 µg/mL. In contrast, the clinical isolate of tetracycline-resistant Staphylococcus aureus was the most sensitive strain (MIC 128 µg/mL). The major constituents of the EO were 15,16-dinorlabda-8(17),11-dien-13-one (24.63/15.78%), followed by ambrial (16.12/10.97%), 13-nor-eremophil-1(10)-en-11-one (7.16/6.21%), 15,16-dinorlabda-8(17),12-dien-14-al (6.61/11.57%), and aromadendrene oxide (5.98/3.77%). These results propose C. mangga rhizome EO as a promising agent for developing natural-based anti-infective preparations.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"106 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139859634","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Exploring Bioactive Phytochemicals in Gymnema sylvestre: Biomedical Uses and Computational Investigations","authors":"U. Muddapur, Samiksha Manjunath, Yahya S. Alqahtani, I. Shaikh, A. Khan, B. A. Mannasaheb, Deepak A. Yaraguppi, S. More","doi":"10.3390/separations11020050","DOIUrl":"https://doi.org/10.3390/separations11020050","url":null,"abstract":"The main objective of this research was to perform Gymnema sylvestre (Asclepiadaceae) extract’s phytochemical screening and identify its therapeutic potential. Using a Soxhlet apparatus, the powdered plant material was extracted using ethyl acetate. The preliminary phytochemical analysis confirmed the presence of alkaloids, flavonoids, phenols, glycosides, and steroids. Gas chromatography–mass spectroscopy analysis of the extract was performed and confirmed the presence of 11 compounds. As per the quantitative analysis, the extract exhibited a phenolic content of 948 µg gallic acid equivalent/g dry weight, a total flavonoid content of 398 µg quercetin equivalent/g dry weight, and an alkaloid content of 487 µg atropine equivalent/g dry weight. As per the in vitro cytotoxicity test using A549 cells, the IC50 (half-maximal inhibitory concentration) value for the extract was found to be 76.06 ± 1.26 µg/mL, indicating its cytotoxic effect on the cells. The ethyl acetate extract showed significant antibacterial efficacy, as evidenced by a zone of clearance measuring 3 mm against Escherichia coli and 6 mm against Bacillus subtilis. For anthelmintic activity, the earthworm paralysis time induced by G. sylvestre extract (10 mg/mL) was 28.13 ± 0.8 min, and the time of death was 68.21 ± 1.72 min. In comparison, the reference drug, piperazine citrate (10 mg/mL), caused paralysis in 22.18 ± 1.02 min and resulted in death at 66.22 ± 2.35 min. Similarly, the coagulation time was notably prolonged, with blood clot formation observed at 1 min and 40 s, at a concentration of 1 mg/mL, which underscores the potential anticoagulant or hemostatic modulation properties of G. sylvestre extract. The test extract showed good inhibition of alpha-amylase activity and exhibited an IC50 value of 15.59 µg/mL. The IC50 value for DPPH (2,2-diphenyl-1-picrylhydrazyl)-scavenging activity for the extract was 19.19 µg/mL. Based on the GCMS results, the compound 2,7-dimethyl-undecane was selected for its anticancer potential. Docking studies were conducted with the epidermal growth factor receptor (EGFR) protein, specifically the 5WB7 variant associated with lung cancer. The docking score was −4.5, indicating a potential interaction. Key interaction residues such as ASN328, VAL350, and THR358 were identified. Overall, this research provides valuable insights into the phytochemical composition and diverse biological activities of G. sylvestre extract, offering a foundation for further exploration of its medicinal and pharmacological potential.","PeriodicalId":510456,"journal":{"name":"Separations","volume":"16 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139799070","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}